CN101955547A - Method for comprehensively extracting changium smyrnioide polysaccharides and amino acid - Google Patents
Method for comprehensively extracting changium smyrnioide polysaccharides and amino acid Download PDFInfo
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- CN101955547A CN101955547A CN2010101829447A CN201010182944A CN101955547A CN 101955547 A CN101955547 A CN 101955547A CN 2010101829447 A CN2010101829447 A CN 2010101829447A CN 201010182944 A CN201010182944 A CN 201010182944A CN 101955547 A CN101955547 A CN 101955547A
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Abstract
The invention relates to a method for comprehensively extracting changium smyrnioide polysaccharides and changium smyrnioide amino acid. The method comprises the following steps of: extracting with hot water and acid water, filtering, putting the extract on a cation exchange resin column, collecting effluent liquid which is not adsorbed by resin, adding high-concentration ethanol into the effluent liquid, leaching precipitates, washing with acetone and performing freeze drying so as to obtain the changium smyrnioide polysaccharides; and eluting the resin with ammonia water, adjusting pH, separating an emulsion liquid membrane, concentrating an organic nanofiltration membrane and drying so as to obtain the changium smyrnioide amino acid. The method has the advantages of mild reaction condition, a small amount of polysaccharide loss, high amino acid activity, short process path, energy saving and suitability for mass production.
Description
Technical field:
The invention belongs to the field of Chinese medicines, relate to a kind of comprehensive extraction Root of Medicinal Changium polysaccharide and amino acid whose method.
Background technology:
Root of Medicinal Changium is the dry root of samphire Root of Medicinal Changium Changium smyrnioides Wolff.Be used for " tonifying lung gas, logical descending " (" new compilation of materia medica "); " nourishing blood to promote the production of body fluid, clearing heat and detoxicating " (" it is former that book on Chinese herbal medicine is asked "); " warm spleen, it is wet to reduce phlegm, suppressing liver-wind " (" medicine materical crude slice is newly joined ").Root of Medicinal Changium polysaccharide and amino acid are its activeconstituents, play an important role on drug effect.Studies show that, Root of Medicinal Changium and polysaccharide thereof have certain strengthen the body resistance to consolidate the constitution, enhancing immunity and the effect of adaptation former state, on diseases such as anti-curing cancers and infection, the potential using value is arranged.Root of Medicinal Changium can be regulated immunologic function by toughener, has the strengthening by means of tonics effect, and the energy reducing blood-fat, hepatic cholagogic, kobadrin.But the survival time of Root of Medicinal Changium decocting liquid and polysaccharide significant prolongation potassium cyanide poisoning mouse can be resisted the chemical anoxic, prolongs the mouse hot environment survival time, improves high-temperature resistance.Gavage carry in Root of Medicinal Changium water extract and the Root of Medicinal Changium root asparagine all can extremely significantly increase the phenol red excretion of mouse tracheae, can obviously promote frog ciliary movement, and can extremely significantly suppress the cough number of times that ammonia spraying causes, the cavy asthma of breathing heavily is drawn by 2% Ovisot and 0.2% histamine phosphate significant inhibitory effect.Root of Medicinal Changium polysaccharide and water body also all can increase the weight of normal mouse thymus gland and spleen.Mouse carbon clearance speed is obviously improved, promote the phagocytic function of reticuloendothelial system.Also can be very high heatstroke of normal mouse white corpuscle and lymphocyte number, and can resist that total white blood cells and lymphocyte number reduce due to the hydrocortisone.Increase peripheral blood ANAE+ lymphocyte positive percentage.This shows that Root of Medicinal Changium has the wide development prospect, therefore, it is significant that Root of Medicinal Changium polysaccharide and amino acid are carried out the extraction separation purifying.
Current extraction, purifying Root of Medicinal Changium polysaccharide technology, mainly by following several: 1) 95% extraction using alcohol, residue water is carried, concentrating under reduced pressure decocting liquid, refrigeration, centrifugal, throw out is handled the final vacuum drying through ethanol, acetone, ether, water-soluble, Tricholroacetic Acid removes albumen, dialysis, (" separation, purifying and the physico-chemical properties thereof of assay determination Root of Medicinal Changium polysaccharide " that Wang Yashu etc. deliver) such as dialyzate concentrating under reduced pressure, centrifugal, DEAE-cellulose chromatographies.2) water extract-alcohol precipitation, through enzyme process and Sevag method destarch, pectin and protein, the dialysis back is gone up the Sepharose-4B post and is separated (Zhang Linwei, Wu Dongru, Zhao's flag is flat, etc. medicinal plant Root of Medicinal Changium STUDY ON POLYSACHAROSE [J]. University of Anhui's journal (natural science edition), 1996,20 (3): 95-100.).3) sherwood oil, 95% alcohol reflux, residue water is again carried, and the Sevage method is removed albumen, adding alcohol is 80% to containing the alcohol amount, refrigeration (Du Qing, Qin Minjian, Guo Qiaosheng. Root of Medicinal Changium polysaccharide extracting process research [J]. modern Chinese herbal medicine research and practice, 2005,19 (4): 51-53.).Problems such as aforesaid method exists step complexity and cost height, and preparation amount is little, and active polysaccharide is low.Because therefore the existing problem of said extracted purification technique need be improved.
Summary of the invention:
1, goal of the invention: purpose of the present invention just is to provide a kind of and is applicable to industrial production, comprehensively extracts Root of Medicinal Changium polysaccharide and amino acid whose method.
2, technical scheme:
A kind of comprehensive extraction Root of Medicinal Changium polysaccharide and amino acid whose method is characterized in that may further comprise the steps:
(1) extract: the Root of Medicinal Changium root is cleaned, shave, with 8-12 times of hot-water soak, heated and boiled was extracted 2-3 hour, filtered, and kept filtrate; Residue adds the 0.1-0.5mol/LHCl solution that 4-8 doubly measures, and extracts 0.5-1 hour in 30-50 ℃ of constant temperature, filters, and repeats aforesaid operations 1-2 time, merging filtrate;
(2) ion exchange resin separates: above-mentioned filtrate by Zeo-karb, is used earlier the deionized water wash-out, elutriant A is added the 70-95% edible ethanol, leach precipitation, add washing with acetone, be drying to obtain the Root of Medicinal Changium polysaccharide; Use the ammoniacal liquor wash-out again, collect elutriant B, standby;
(3) preparation of milk sap: by membrane solvent edible oil: tensio-active agent Span 80: the volume ratio of phosphoric acid ester carrier=(30-50): (2-10): (2-8) mix, press in mixture (1-5): it is the hydrochloric acid soln of 0.2-0.5mol/L that 1 volume ratio adds concentration, stir 2-5min at 5000-15000r/min, make stable w/o type milk sap;
(4) amino acid whose purifying: elutriant B is transferred pH to 2-5, with milk sap according to certain volume ratio (10: 1-10: 4) add in the extractor, extract 5-15min in the 100-500r/min stirring at low speed, change milk sap in separating funnel standing demix, tell milk sap, divide oil-yielding stratum behind the heating in water bath breakdown of emulsion, gained water vacuum lyophilization is promptly got Root of Medicinal Changium amino acid.
The mass ratio of repetitive operation hot water and crude drug is 2 in the step (1): 1-4: 1; HCl solution add-on is a 4-6 times of residue quality.
Eluent is the 3-6 column volume for the deionized water elution volume in the step (2), and elution speed is 0.8-4BV/h.
Ammonia concn is 0.5-5mol/L. in the step (2), is eluted to till the no amino acid reaction.
In sum, the present invention has mild condition, polysaccharide loss is few, amino acid active is high, operation is few, and preparation amount is big, is applicable to fields such as medicine, food.
Embodiment:
The present invention is described further below in conjunction with embodiment.
Embodiment 1:
(1) preparation of Root of Medicinal Changium extracting solution: with Root of Medicinal Changium undercut thin slice, take by weighing 10g and add 120ml hot-water soak 0.5h, heated and boiled is extracted 2h, filter, keep filtrate, residue adds 5 times of amount 0.5mol/LHCl, extract 1h in 40 ℃ of constant temperature, filter, filter residue adds 3 times of little boiling of volume hot water again and extracts 1h, filters, filter residue adds 3 times of amount 0.5mol/LHCl, extract 0.5h in 40 ℃ of constant temperature, filter merging filtrate.
(2) ion exchange resin separates: above-mentioned filtrate by D85 macropore weakly acidic cation-exchange resin post, is used earlier the deionized water wash-out, get elutriant A, use 5mol/L ammoniacal liquor wash-out again, get elutriant B.
(3) purifying of polysaccharide: elutriant A is added 95% ethanol, and the leaching precipitation is used washing with acetone, and spraying drying promptly gets Root of Medicinal Changium polysaccharide sample 1.03g, and Root of Medicinal Changium polysaccharide massfraction is 80.7%, and yield accounts for 10.3% of medicinal material dry weight.
(4) preparation of milk sap: get membrane solvent edible oil 18mL, tensio-active agent 4mL, phosphoric acid ester carrier 2.5mL, the three is mixed, get the hydrochloric acid soln of this mixture of 20mL, stir 3min, promptly get stable w/o type milk sap at 8000r/min by 3: 1 volume ratio adding 7mL0.2mol/L.
(5) amino acid whose purifying: elutriant B is transferred pH to 3, is to add in extractor at 10: 3 the amino acid crude extract of pH=3 and milk sap according to the whey volume ratio, under the low speed of 220r/min, stir and extract 8min, change milk sap in separating funnel standing demix, tell milk sap, divide oil-yielding stratum behind the heating in water bath breakdown of emulsion, gained water vacuum lyophilization promptly gets Root of Medicinal Changium amino acid 0.8mg.
Embodiment 2:
(1) preparation of Root of Medicinal Changium extracting solution: with Root of Medicinal Changium undercut thin slice, take by weighing 2kg and add 20L hot-water soak 1h, heated and boiled is extracted 2.5h, filter, keep filtrate, residue adds 6 times of amount 0.2mol/LHCl, extract 1h in 40 ℃ of constant temperature, filter, filter residue adds 4 times of little boiling of volume hot water again and extracts 1h, filters, filter residue adds 3 times of amount 0.2mol/LHCl, extract 0.5h in 40 ℃ of constant temperature, filter merging filtrate;
(2) ion exchange resin separates: above-mentioned filtrate by D85 macropore weakly acidic cation-exchange resin post, is used earlier the deionized water wash-out, get elutriant A, use 2mol/L ammoniacal liquor wash-out again, get elutriant B.
(3) purifying of polysaccharide: elutriant A is added 70% ethanol, and the leaching precipitation is used washing with acetone, and spraying drying promptly gets Root of Medicinal Changium polysaccharide sample 246g, and Root of Medicinal Changium polysaccharide massfraction is 85.7%, and yield accounts for 12.3% of medicinal material dry weight.
(3) preparation of milk sap: get membrane solvent edible oil 2.5L, tensio-active agent 0.7L, phosphoric acid ester carrier 0.8L, the three is mixed, this mixture stirs 5min by the hydrochloric acid soln of 2: 1 volume ratio adding 0.2mol/L at 9000r/min, promptly gets stable w/o type milk sap.
(4) amino acid whose purifying: elutriant B is transferred pH to 3, is to add in extractor at 10: 1 the amino acid crude extract of pH=3 and milk sap according to the whey volume ratio, under the low speed of 300r/min, stir and extract 15min, change milk sap in separating funnel standing demix, tell milk sap, divide oil-yielding stratum behind the heating in water bath breakdown of emulsion, gained water vacuum lyophilization promptly gets Root of Medicinal Changium amino acid/11 68mg.
Embodiment 3:
(1) preparation of Root of Medicinal Changium extracting solution: with Root of Medicinal Changium undercut thin slice, take by weighing 5kg and add 40L hot-water soak 40min, heated and boiled is extracted 3h, filter, keep filtrate, residue adds 8 times of amount 0.4mol/LHCl, extract 1h in 40 ℃ of constant temperature, filter, filter residue adds 3 times of little boiling of volume hot water again and extracts 1h, filters, filter residue adds 4 times of amount 0.4mol/LHCl, extract 0.5h in 40 ℃ of constant temperature, filter merging filtrate;
(2) ion exchange resin separates: above-mentioned filtrate by D85 macropore weakly acidic cation-exchange resin post, is used earlier the deionized water wash-out, get elutriant A, use 1mol/L ammoniacal liquor wash-out again, get elutriant B.
(3) purifying of polysaccharide: elutriant A is added 85% ethanol, and the leaching precipitation is used washing with acetone, and spraying drying promptly gets Root of Medicinal Changium polysaccharide sample 572g, and Root of Medicinal Changium polysaccharide massfraction is 83.7%, and yield accounts for 11.4% of medicinal material dry weight.
(4) preparation of milk sap: get membrane solvent edible oil 43L, tensio-active agent 3.5L, phosphoric acid ester carrier 5.5L, the three is mixed, this mixture stirs 4min by the hydrochloric acid soln of 4: 1 volume ratio adding 0.5mol/L at 10000r/min, promptly gets stable w/o type milk sap.
(5) amino acid whose purifying: elutriant B is transferred pH to 3, is to add in extractor at 10: 4 the amino acid crude extract of pH=3 and milk sap according to the whey volume ratio, under the low speed of 280r/min, stir and extract 10min, change milk sap in separating funnel standing demix, tell milk sap, divide oil-yielding stratum behind the heating in water bath breakdown of emulsion, gained water vacuum lyophilization promptly gets Root of Medicinal Changium amino acid 420mg.
Claims (4)
1. one kind is comprehensively extracted Root of Medicinal Changium polysaccharide and amino acid whose method, it is characterized in that may further comprise the steps:
(1) extract: the Root of Medicinal Changium root is cleaned, shave, with 8-12 times of hot-water soak, heated and boiled was extracted 2-3 hour, filtered, and kept filtrate; Residue adds the 0.1-0.5mol/LHCl solution that 4-8 doubly measures, and extracts 0.5-1 hour in 30-50 ℃ of constant temperature, filters, and repeats aforesaid operations 1-2 time, merging filtrate;
(2) ion exchange resin separates: above-mentioned filtrate by Zeo-karb, is used earlier the deionized water wash-out, elutriant A is added the 70-95% edible ethanol, leach precipitation, add washing with acetone, be drying to obtain the Root of Medicinal Changium polysaccharide; Use the ammoniacal liquor wash-out again, collect elutriant B, standby;
(3) preparation of milk sap: by membrane solvent edible oil: tensio-active agent Span 80: the volume ratio of phosphoric acid ester carrier=(30-50): (2-10): (2-8) mix, press in mixture (1-5): it is the hydrochloric acid soln of 0.2-0.5mol/L that 1 volume ratio adds concentration, stir 2-5min at 5000-15000r/min, make stable w/o type milk sap;
(4) amino acid whose purifying: elutriant B is transferred pH to 2-5, with milk sap according to certain volume ratio (10: 1-10: 4) add in the extractor, extract 5-15min in the 100-500r/min stirring at low speed, change milk sap in separating funnel standing demix, tell milk sap, divide oil-yielding stratum behind the heating in water bath breakdown of emulsion, gained water vacuum lyophilization is promptly got Root of Medicinal Changium amino acid.
2. the method for claim 1 is characterized in that in the step (1) that the mass ratio of hot water and crude drug is 2 in the repetitive operation: 1-4: 1; HCl solution add-on is a 4-6 times of residue quality.
3. the method for claim 1 is characterized in that eluent is the 3-6 column volume for the deionized water elution volume in the step (2), and elution speed is 0.8-4BV/h.
4. the method for claim 1 is characterized in that ammonia concn is 0.5-5mol/L. in the step (2), is eluted to till the no amino acid reaction.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109315773A (en) * | 2018-11-07 | 2019-02-12 | 中国科学院兰州化学物理研究所 | A kind of fructus lycii Radix Codonopsis strengthen immunity health food and preparation method thereof |
| CN109315739A (en) * | 2018-11-07 | 2019-02-12 | 中国科学院兰州化学物理研究所 | A kind of fructus lycii Bee Pollen antineoplastic health product and preparation method thereof |
| CN112827211A (en) * | 2021-02-07 | 2021-05-25 | 三益创价生物科技(深圳)有限公司 | Method for extracting high-content amino acid from gynura segetum and extract |
| CN114181388A (en) * | 2021-11-30 | 2022-03-15 | 河北圣雪大成制药有限责任公司 | Method for extracting polylysine from fermentation liquor |
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2010
- 2010-05-26 CN CN2010101829447A patent/CN101955547A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109315773A (en) * | 2018-11-07 | 2019-02-12 | 中国科学院兰州化学物理研究所 | A kind of fructus lycii Radix Codonopsis strengthen immunity health food and preparation method thereof |
| CN109315739A (en) * | 2018-11-07 | 2019-02-12 | 中国科学院兰州化学物理研究所 | A kind of fructus lycii Bee Pollen antineoplastic health product and preparation method thereof |
| CN112827211A (en) * | 2021-02-07 | 2021-05-25 | 三益创价生物科技(深圳)有限公司 | Method for extracting high-content amino acid from gynura segetum and extract |
| CN114181388A (en) * | 2021-11-30 | 2022-03-15 | 河北圣雪大成制药有限责任公司 | Method for extracting polylysine from fermentation liquor |
| CN114181388B (en) * | 2021-11-30 | 2023-12-01 | 河北圣雪大成制药有限责任公司 | Method for extracting polylysine from fermentation liquor |
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Application publication date: 20110126 |